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Here, we demonstrate that the controlled thermal decomposition of molybdenum(II) acetate under vacuum provides a simple solid-state route for obtaining monoclinic MoO2 nanoparticles and hexagonal \u03b2-Mo2C with tunable morphology. Structural, morphological, and thermal analyses revealed a three-stage transformation pathway: (i) precursor degradation and amorphization between 300 and 400 \u00b0C; (ii) nucleation and crystallization of monoclinic MoO2 between 500 and 700 \u00b0C, yielding spherical nanoparticles with an average diameter of 23 \u00b1 7.9 nm; and (iii) formation of vertically oriented MoO2\/\u03b2-Mo2C microflakes at 800 \u00b0C, evidencing nanoparticle coalescence and the partial conversion of MoO2 into the \u03b2-Mo2C phase. Time-Differential Perturbed Angular Correlation (TDPAC) spectroscopy, using the 111In(111Cd) probe, provided atomic-scale information on local electric field gradients, enabling the direct identification of amorphous and crystalline MoO2 environments while revealing the role of defects, oxygen vacancies, and surface heterogeneities during phase evolution. These findings establish molybdenum(II) acetate as an effective precursor for the synthesis of molybdenum-based nanostructures and provide a multiscale understanding, spanning atomic to micrometer length scales, of the mechanisms governing the formation of MoO2 and \u03b2-Mo2C. Furthermore, the results indicate that carbonaceous species generated during precursor decomposition promote a coupled carbothermal reduction\u2013carburization pathway, leading to the formation of \u03b2-Mo2C.<\/jats:p>","DOI":"10.1021\/acsomega.6c04468","type":"journal-article","created":{"date-parts":[[2026,8,17]],"date-time":"2026-08-17T10:02:03Z","timestamp":1786960923000},"page":"51371-51387","source":"Crossref","is-referenced-by-count":1,"title":["Thermal Decomposition\nof Molybdenum(II) Acetate as\na Controlled Route to MoO2 and Mo2C Nanostructures:\nStructural, Morphological, and Atomic-Scale Insights"],"prefix":"10.1021","volume":"11","author":[{"given":"Katiusse","family":"Soares de Souza","sequence":"first","affiliation":[{"name":"Instituto de Pesquisas Energe\u0301ticas e Nucleares , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 05508-000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Crystian W. C.","family":"Silva","sequence":"additional","affiliation":[{"name":"Instituto de Pesquisas Energe\u0301ticas e Nucleares , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 05508-000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Anastasia","family":"Burimova","sequence":"additional","affiliation":[{"name":"Instituto de Pesquisas Energe\u0301ticas e Nucleares , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 05508-000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Levy","family":"Scalise","sequence":"additional","affiliation":[{"name":"Instituto de Pesquisas Energe\u0301ticas e Nucleares , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 05508-000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gabriel","family":"Cabrera-Pasca","sequence":"additional","affiliation":[{"name":"Universidade Federal do Para\u0301 , , ,","place":["Abaetetuba, Para\u0301, Brazil, 09210-580"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Juliana","family":"Schell","sequence":"additional","affiliation":[{"name":"European Organization for Nuclear Research (CERN) , ,","place":["Geneva, Switzerland, CH-1211"]},{"name":"University of Duisburg-Essen , , ,","place":["Essen, Germany, 45141"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Larissa","family":"Otubo","sequence":"additional","affiliation":[{"name":"Instituto de Pesquisas Energe\u0301ticas e Nucleares , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 05508-000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-4499-5949","authenticated-orcid":true,"given":"Artur Wilson","family":"Carbonari","sequence":"additional","affiliation":[{"name":"Instituto de Pesquisas Energe\u0301ticas e Nucleares , , , ,","place":["Sa\u0303o Paulo, Sa\u0303o Paulo, Brazil, 05508-000"]},{"name":"European Organization for Nuclear Research (CERN) , Esplanade des Particules 1 , ,","place":["Meyrin, Switzerland, 1217"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,8,17]]},"reference":[{"key":"2026090307200596900_cit1","doi-asserted-by":"publisher","first-page":"8819","DOI":"10.1016\/j.ijhydene.2022.11.330","article-title":"In-situ \u201cencapsulation\u201d\nof Mo:Mo2C with nano-mosaic structure on wood-derived carbon\nfor hydrogen evolution reaction","volume":"48","author":"Hu","year":"2023","journal-title":"Int. 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Chem."},{"key":"2026090307200596900_cit24","doi-asserted-by":"publisher","first-page":"106358","DOI":"10.1016\/j.ijrmhm.2023.106358","article-title":"Preparation of ultrafine Mo powder\nby the H2 reduction of MoO2: Parameter optimization,\nreaction kinetic, and its reduction mechanism","volume":"116","author":"Li","year":"2023","journal-title":"Int. J. Refract. Metals Hard Mater."},{"key":"2026090307200596900_cit25","doi-asserted-by":"publisher","first-page":"1435","DOI":"10.1016\/j.ijhydene.2019.11.008","article-title":"Size-controlled\nsynthesis of Mo powders via hydrogen reduction of MoO2 powders\nwith the assistance of Mo nuclei","volume":"45","author":"Zhang","year":"2020","journal-title":"Int. J. Hydrogen\nEnergy"},{"key":"2026090307200596900_cit26","doi-asserted-by":"publisher","first-page":"384","DOI":"10.1016\/j.jallcom.2006.10.154","article-title":"Effect of\nheat-treatment on cobalt\u2013molybdenum\nsystem","volume":"452","author":"Kashif","year":"2008","journal-title":"J. Alloys Compd."},{"key":"2026090307200596900_cit27","doi-asserted-by":"publisher","first-page":"21387","DOI":"10.1021\/acs.jpcc.3c05159","article-title":"Thermal\nReduction of MoO3 Particles and Formation of MoO2 Nanosheets Monitored by In Situ Transmission Electron Microscopy","volume":"127","author":"Chen","year":"2023","journal-title":"J. Phys. Chem. C"},{"key":"2026090307200596900_cit28","doi-asserted-by":"publisher","first-page":"1853","DOI":"10.1021\/cm9800229","article-title":"Effect of the Reactive Gas on the\nSolid-State Transformation of Molybdenum Trioxide to Carbides and\nNitrides","volume":"10","author":"Li","year":"1998","journal-title":"Chem. 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Chem. Rev."},{"key":"2026090307200596900_cit34","doi-asserted-by":"publisher","first-page":"16869","DOI":"10.1021\/jp804413a","article-title":"Thermal Stability and\nReducibility of Oxygen-Containing Functional Groups on Multiwalled\nCarbon Nanotube Surfaces: A Quantitative High-Resolution XPS and TPD\/TPR\nStudy","volume":"112","author":"Kundu","year":"2008","journal-title":"J. Phys. Chem. C"},{"key":"2026090307200596900_cit35","doi-asserted-by":"publisher","first-page":"108900","DOI":"10.1016\/j.cclet.2023.108900","article-title":"Recent advances\nin iron-based sulfides electrocatalysts for oxygen and hydrogen evolution\nreaction","volume":"35","author":"Mei","year":"2024","journal-title":"Chin. Chem. Lett."},{"key":"2026090307200596900_cit36","doi-asserted-by":"publisher","first-page":"110","DOI":"10.1016\/j.tca.2014.02.020","article-title":"An investigation of the thermal decomposition of silver\nacetate as a precursor for nano-sized Ag-catalyst","volume":"581","author":"Abu-Zied","year":"2014","journal-title":"Thermochim. Acta"},{"key":"2026090307200596900_cit37","doi-asserted-by":"publisher","first-page":"8841","DOI":"10.1021\/acs.jpcc.6b02377","article-title":"Thermal decomposition\nof silver acetate:\nphysico-geometrical kinetic features and formation of silver nanoparticles","volume":"120","author":"Nakano","year":"2016","journal-title":"J. Phys. Chem. C"},{"key":"2026090307200596900_cit38","doi-asserted-by":"publisher","first-page":"239","DOI":"10.14233\/ajchem.2022.23495","article-title":"Thermal decomposition\nof copper acetate at various temperature and time to form copper oxide\/copper\nnanoparticles","volume":"34","author":"Sibokoza","year":"2021","journal-title":"Asian J. Chem."},{"key":"2026090307200596900_cit39","doi-asserted-by":"publisher","first-page":"139084","DOI":"10.1016\/j.molstruc.2024.139084","article-title":"NiO nanoparticles\nby thermal decomposition of complex and evaluation of the structural,\nmorphological, and optical properties","volume":"1317","author":"Onwudiwe","year":"2024","journal-title":"J. Mol.\nStruct."},{"key":"2026090307200596900_cit40","doi-asserted-by":"publisher","first-page":"117","DOI":"10.1007\/s10973-008-9173-1","article-title":"An investigation\nof the thermal decomposition\nof gold acetate","volume":"95","author":"Bakrania","year":"2009","journal-title":"J. Therm. Anal. Calorim."},{"key":"2026090307200596900_cit41","doi-asserted-by":"publisher","first-page":"2768","DOI":"10.1107\/S0567740874008053","article-title":"Dimolybdenum\ntetraacetate","volume":"30","author":"Cotton","year":"1974","journal-title":"Acta Crystallogr. Sect. B Struct.\nCrystallogr. Cryst. Chem."},{"key":"2026090307200596900_cit42","doi-asserted-by":"publisher","first-page":"921","DOI":"10.1021\/ja01082a046","article-title":"The Molecular Structure of Molybdenum(II) Acetate","volume":"87","author":"Lawton","year":"1965","journal-title":"J. Am. Chem. 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